Recently, two-dimensional nanomaterials have received great attention in the field of electrochemical applications because of their outstanding physicochemical properties. In this research, we developed vanadium carbide entrapped on graphitic carbon nitride nanosheets (VC/g-CN NSs) as a highly efficient electrocatalyst for the determination of furazolidone (FZD) in biological samples. The VC/g-CN NSs nanocomposite was systematically characterized by various analytical and spectroscopic techniques. The electrochemical performance of the VC/g-CN NSs-modified glassy carbon electrode (GCE) for the FZD detection was studied by the cyclic voltammetry and amperometric methods. On the one hand, the fabricated electrode offers numerous active sites with the large electron-transfer rate and the rapid mass transport ability to enhance the electrochemical activity toward the FZD detection. Under the optimization conditions, the VC/g-CN NSs modified electrode showed a wide detection range (0.004−141 μM), very low detection limit (0.5 nM), excellent selectivity, and reproducibility. Compared to the previous studies, the fabricated VC/g-CN NSs/GCE achieves the lowest limit of detection and the widest linear rangetoward the FZD detection. Furthermore, the fabricated sensor was successfully applied to determine FZD in the biological samples with satisfactory results.